CN103305788A - Preparation method of antimony assistant for oriented silicon steel - Google Patents
Preparation method of antimony assistant for oriented silicon steel Download PDFInfo
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- CN103305788A CN103305788A CN2013102255462A CN201310225546A CN103305788A CN 103305788 A CN103305788 A CN 103305788A CN 2013102255462 A CN2013102255462 A CN 2013102255462A CN 201310225546 A CN201310225546 A CN 201310225546A CN 103305788 A CN103305788 A CN 103305788A
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Abstract
The invention relates to manufacturing of oriented silicon steel, and in particular relates to preparation of an antimony assistant for oriented silicon steel, and more particularly relates to a preparation method of the antimony assistant for oriented silicon steel. The method comprises the following steps: adding titanium dioxide, antimonous oxide and softened water into a reaction kettle, and starting stirring and opening a steam valve to heat, wherein the solid-liquid mass ratio of the titanium dioxide and antimonous oxide to the softened water is 1: (25-30); carrying out filter pressing on reactants obtained in the reaction kettle to obtain filter cakes; drying the filter cakes in a drying box at 200-250 DEGX for 3.0-4.0 hours; and crushing the dried filter cakes, and screening the obtained powder by a 320-mesh sieve frame, wherein the residue on sieve is less or equal to 0.1% based on total weight of powder. According to the preparation method, the problems that in manufacturing of oriented silicon steel, an adopted imported antimony assistant is high in cost and hard to carry out exchange of skills, and the antimony assistant has poor effects of improving induction of oriented silicon steel and reducing iron loss are solved.
Description
Technical field
The present invention relates to the manufacturing of oriented silicon steel, relate in particular to oriented silicon steel with the preparation of antimony auxiliary agent, be specially the preparation method that a kind of oriented silicon steel is used the antimony auxiliary agent.
Background technology
At present, the oriented silicon steel specification is developed to high magnetic strength (Hi-B) by general oriented silicon steel, and raising oriented silicon steel magnetic strength and reduction iron loss are one key subjects.High magnetic induction grain-oriented silicon steel is in manufacturing processed, in order to increase silicon-dioxide and magnesian synthesising reacting speed in the steel plate, improve magnesian dispersiveness and reactivity, improve the sticking power of underlayer insulating film layer Magnesium Silicate q-agent, Sb is infiltrated on secondary recrystallization front spring surface, can strengthen restraint, promotes top layer subgrain development, improve the electromagnetic performance of oriented silicon steel, oriented silicon steel manufacturing firm generally adds the antimony auxiliary agent in oriented silicon steel both at home and abroad.Present Domestic prepares the antimony auxiliary agent of high magnetic induction grain-oriented silicon steel enterprise such as Baosteel, the equal import of Wuhan Iron and Steel Plant Japan outward, in actual use, has that production cost is high, exchange of technology is difficult, and buying and capital settlement comparatively bother harsh problem; Antimony auxiliary agent from Japanese import, viscosity large because of its granularity is low simultaneously exists the problem that the oriented silicon steel magnetic strength improves, iron loss reduces weak effect.Therefore the oriented silicon steel that domesticizes is very urgent with the antimony auxiliary agent.
Summary of the invention
The cost that adopts import antimony auxiliary agent to exist in the oriented silicon steel manufacturing is high, exchange of technology is difficult and the problem of import antimony auxiliary agent raising oriented silicon steel magnetic strength and reduction iron loss weak effect in order to solve in the present invention, and a kind of oriented silicon steel preparation method of antimony auxiliary agent is provided.
The present invention adopts following technical scheme to realize: a kind of oriented silicon steel preparation method of antimony auxiliary agent may further comprise the steps:
The softening water of specific conductivity≤10 μ s/cm is squeezed into reactor, open and stir, stirring velocity is 200-250r/min, in reactor, add titanium dioxide 2.9-3.0 part and antimonous oxide 7.0-7.1 part, the solid-liquid mass ratio is adjusted to 1:25-30 in the reactor, and the titanium dioxide purity that adds is more than or equal to 98%, the amount of the contained water solubles is less than or equal to 1%, the purity of antimonous oxide is more than or equal to 99.8%, the amount of contained ferric oxide is less than or equal to 0.002%, then open steam valve heating, Heating temperature is 55-70 ℃, heat-up time 1.0h-2.0h;
The reactant that obtains in the reactor is carried out press filtration, obtain filter cake;
In the loft drier inner drying, drying temperature is 200-250 ℃ with above-mentioned filter cake, and be 3.0-4.0h time of drying;
Dried filter cake is pulverized, and after requiring the gained powder to be the screening of 320 purpose screen frames with the order number, screenings accounts for the powder total amount and is less than or equal to 0.1%.
The invention provides a kind of oriented silicon steel preparation method of antimony auxiliary agent, the method is raw material with titanium dioxide and antimonous oxide, makes oriented silicon steel antimony auxiliary agent; In manufacturing processed, utilized the steam foam theory to improve the viscosity of raw material, and steam-heated temperature is optimized, because if Heating temperature is lower, the powder viscosity that then is made into is lower, if Heating temperature is higher, the powder granule that is made into is larger, can not reach the requirement of technique, and viscosity is also lower, so the steam heating temperature selects 55-70 ℃, has guaranteed that powder has higher viscosity; Also the mass ratio of raw material and softening water has been made preferably, if softening water very little, then the water solubles is processed unclean in the titanium dioxide, if softening water is too many, then press filtration, the drying step very complicated that becomes is selected raw material and softening water quality than being 1:25-30, guaranteeing that the water solubles is processed as much as possible falls, and used softening water specific conductivity≤10 μ s/cm, the solubleness of the water solubles is high like this, and the water solubles can be removed as much as possible; Drying temperature also is preferably 200-250 ℃, otherwise when time of drying fixedly the time, if temperature is too high, the powder granule of making is thicker, can not reach the requirement of technique; Utilizing at last the order number is that 320 purpose screen frames are strictly controlled the powder granularity of making, and guarantees that powder granularity reaches processing requirement, thereby guarantees the result of use of antimony auxiliary agent.
The cost that the invention solves employing import antimony auxiliary agent existence in the oriented silicon steel manufacturing is high, exchange of technology is difficult and the problem of import antimony auxiliary agent raising oriented silicon steel magnetic strength and reduction iron loss weak effect, the antimony auxiliary agent that also present method is made compares comparative data such as following table with Japanese similar antimony auxiliary agent:
By data sheet as can be known, the antimony auxiliary agent granularity that present method makes is much smaller than the similar antimony auxiliary agent of Japan, and viscosity is greater than the similar antimony auxiliary agent of Japan, the antimony auxiliary agent sticking power that present method makes is the B level, more easily be attached to surface of silicon steel, so that iron loss of oriented silicon steel by utilizing is less than 1W/Kg, magneticflux-density is greater than 1.930T; In addition, also entrust Wuhan Iron and Steel Plant research institute silicon steel that the antimony auxiliary agent is analyzed, analyze to report and draw, the antimony auxiliary agent that interpolation present method makes in the oriented silicon steel manufacturing is compared with the Japanese antimony auxiliary agent of interpolation, adhesion property is good, and oriented silicon steel bottom appearance color is even, does not reveal brilliant phenomenon, magnetic property of oriented silicon steel is strong, the high 2-5% of trade mark rate and the percentage of A-class goods.
In a word, compare with currently available products, oriented silicon steel of the present invention antimony auxiliary agent is raw material production with titanium dioxide, antimonous oxide, three-waste free pollution, and production technique is simple, and cost is lower, but large-scale promotion oriented silicon steel disc uses.
Embodiment
Embodiment one:
A kind of oriented silicon steel preparation method of antimony auxiliary agent may further comprise the steps:
The softening water of specific conductivity≤10 μ s/cm is squeezed into reactor, open and stir, stirring velocity is 200r/min, add 7.1 parts of 2.9 parts of titanium dioxide and antimonous oxides in the reactor, the solid-liquid mass ratio is adjusted to 1:25 in the reactor, and the titanium dioxide purity that adds is more than or equal to 98%, the amount of the contained water solubles is less than or equal to 1%, the purity of antimonous oxide is more than or equal to 99.8%, the amount of contained ferric oxide is less than or equal to 0.002%, then open steam valve heating, Heating temperature is 55 ℃, heat-up time 1.0h;
The reactant that obtains in the reactor is carried out press filtration in plate-and-frame filter press, the filter cake that obtains;
In the loft drier inner drying, drying temperature is 200 ℃ with above-mentioned filter cake, and be 3.0h time of drying;
Dried filter cake obtains powder with the grading machine processing under pulverizer, and after requiring the gained powder to be the screening of 320 purpose screen frames with the order number, screenings accounts for the powder total amount and is less than or equal to 0.1%.
Embodiment two:
A kind of oriented silicon steel preparation method of antimony auxiliary agent may further comprise the steps:
The softening water of specific conductivity≤10 μ s/cm is squeezed into reactor, open and stir, stirring velocity is 210r/min, add 7.0 parts of 3.0 parts of titanium dioxide and antimonous oxides in the reactor, the solid-liquid mass ratio is adjusted to 1:26 in the reactor, and the titanium dioxide purity that adds is more than or equal to 98%, the amount of the contained water solubles is less than or equal to 1%, the purity of antimonous oxide is more than or equal to 99.8%, the amount of contained ferric oxide is less than or equal to 0.002%, then open steam valve heating, Heating temperature is 60 ℃, heat-up times 1.2 h;
The reactant that obtains in the reactor is carried out press filtration in plate-and-frame filter press, obtain filter cake;
In the loft drier inner drying, drying temperature is 210 ℃ with above-mentioned filter cake, and be 3.2h time of drying;
Dried filter cake obtains powder with the grading machine processing under pulverizer, and after requiring the gained powder to be the screening of 320 purpose screen frames with the order number, screenings accounts for the powder total amount and is less than or equal to 0.1%.
Embodiment three:
A kind of oriented silicon steel preparation method of antimony auxiliary agent may further comprise the steps:
The softening water of specific conductivity≤10 μ s/cm is squeezed into reactor, open and stir, stirring velocity is 220r/min, add 7.08 parts of 2.92 parts of titanium dioxide and antimonous oxides in the reactor, and the solid-liquid mass ratio is adjusted to 1:27 in the reactor, and the titanium dioxide purity that adds is more than or equal to 98%, the amount of the contained water solubles is less than or equal to 1%, the purity of antimonous oxide is more than or equal to 99.8%, the amount of contained ferric oxide is less than or equal to 0.002%, then open steam valve heating, Heating temperature is 65 ℃, heat-up time 1.4h;
The reactant that obtains in the reactor is carried out press filtration in plate-and-frame filter press, obtain filter cake;
In the loft drier inner drying, drying temperature is 220 ℃ with above-mentioned filter cake, and be 3.4h time of drying;
Dried filter cake obtains powder with the grading machine processing under pulverizer, and after requiring the gained powder to be the screening of 320 purpose screen frames with the order number, screenings accounts for the powder total amount and is less than or equal to 0.1%.
Embodiment four:
A kind of oriented silicon steel preparation method of antimony auxiliary agent may further comprise the steps:
The softening water of specific conductivity≤10 μ s/cm is squeezed into reactor, open and stir, stirring velocity is 230r/min, add 7.06 parts of 2.94 parts of titanium dioxide and antimonous oxides in the reactor, and the solid-liquid mass ratio is adjusted to 1:28 in the reactor, and the titanium dioxide purity that adds is more than or equal to 98%, the amount of the contained water solubles is less than or equal to 1%, the purity of antimonous oxide is more than or equal to 99.8%, the amount of contained ferric oxide is less than or equal to 0.002%, then open steam valve heating, Heating temperature is 70 ℃, heat-up time 1.6h;
The reactant that obtains in the reactor is carried out press filtration in plate-and-frame filter press, obtain filter cake;
In the loft drier inner drying, drying temperature is 230 ℃ with above-mentioned filter cake, and be 3.6h time of drying;
Dried filter cake obtains powder with the grading machine processing under pulverizer, and after requiring the gained powder to be the screening of 320 purpose screen frames with the order number, screenings accounts for the powder total amount and is less than or equal to 0.1%.
Embodiment five:
A kind of oriented silicon steel preparation method of antimony auxiliary agent may further comprise the steps:
The softening water of specific conductivity≤10 μ s/cm is squeezed into reactor, open and stir, stirring velocity is 240r/min, add 7.04 parts of 2.96 parts of titanium dioxide and antimonous oxides in the reactor, and the solid-liquid mass ratio is adjusted to 1:29 in the reactor, and the titanium dioxide purity that adds is more than or equal to 98%, the amount of the contained water solubles is less than or equal to 1%, the purity of antimonous oxide is more than or equal to 99.8%, the amount of contained ferric oxide is less than or equal to 0.002%, then open steam valve heating, Heating temperature is 57 ℃, heat-up times 1.8 h;
The reactant that obtains in the reactor is carried out press filtration in plate-and-frame filter press, obtain filter cake;
In the loft drier inner drying, drying temperature is 240 ℃ with above-mentioned filter cake, and be 3.8h time of drying;
Dried filter cake obtains powder with the grading machine processing under pulverizer, and after requiring the gained powder to be the screening of 320 purpose screen frames with the order number, screenings accounts for the powder total amount and is less than or equal to 0.1%.
Embodiment six:
A kind of oriented silicon steel preparation method of antimony auxiliary agent may further comprise the steps:
The softening water of specific conductivity≤10 μ s/cm is squeezed into reactor, open and stir, stirring velocity is 250r/min, add 7.02 parts of 2.98 parts of titanium dioxide and antimonous oxides in the reactor, and the solid-liquid mass ratio is adjusted to 1:30 in the reactor, and the titanium dioxide purity that adds is more than or equal to 98%, the amount of the contained water solubles is less than or equal to 1%, the purity of antimonous oxide is more than or equal to 99.8%, the amount of contained ferric oxide is less than or equal to 0.002%, then open steam valve heating, Heating temperature is 68 ℃, heat-up times 2 h;
The reactant that obtains in the reactor is carried out press filtration in plate-and-frame filter press, obtain filter cake;
In the loft drier inner drying, drying temperature is 250 ℃ with above-mentioned filter cake, and be 4h time of drying;
Dried filter cake obtains powder with the grading machine processing under pulverizer, and after requiring the gained powder to be the screening of 320 purpose screen frames with the order number, screenings accounts for the powder total amount and is less than or equal to 0.1%.
Claims (1)
1. an oriented silicon steel is characterized in that may further comprise the steps with the preparation method of antimony auxiliary agent:
The softening water of specific conductivity≤10 μ s/cm is squeezed into reactor, open and stir, stirring velocity is 200-250r/min, in reactor, add titanium dioxide 2.9-3.0 part and antimonous oxide 7.0-7.1 part, the solid-liquid mass ratio is adjusted to 1:25-30 in the reactor, and the titanium dioxide purity that adds is more than or equal to 98%, the amount of the contained water solubles is less than or equal to 1%, the purity of antimonous oxide is more than or equal to 99.8%, the amount of contained ferric oxide is less than or equal to 0.002%, then open steam valve heating, Heating temperature is 55-70 ℃, heat-up time 1.0h-2.0h;
The reactant that obtains in the reactor is carried out press filtration, obtain filter cake;
In the loft drier inner drying, drying temperature is 200-250 ℃ with above-mentioned filter cake, and be 3.0-4.0h time of drying;
Dried filter cake is pulverized, and after requiring the gained powder to be the screening of 320 purpose screen frames with the order number, screenings accounts for the powder total amount and is less than or equal to 0.1%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104217844A (en) * | 2014-09-03 | 2014-12-17 | 南阳市力矩软磁材料科技有限公司 | Silicon steel sheet with low iron loss, low noise, high magnetic flux and high laminating speed and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0841602A (en) * | 1994-08-01 | 1996-02-13 | Kawasaki Steel Corp | Grain-oriented silicon steel sheet excellent in magnetic property and its production |
| JPH08222423A (en) * | 1995-02-13 | 1996-08-30 | Kawasaki Steel Corp | Grain oriented silicon steel plate of low core loss and its manufacture |
| CN1244597A (en) * | 1998-08-07 | 2000-02-16 | 东北大学 | Laser treatment method of orienting the surface of silicon steel |
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2013
- 2013-06-07 CN CN201310225546.2A patent/CN103305788B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0841602A (en) * | 1994-08-01 | 1996-02-13 | Kawasaki Steel Corp | Grain-oriented silicon steel sheet excellent in magnetic property and its production |
| JPH08222423A (en) * | 1995-02-13 | 1996-08-30 | Kawasaki Steel Corp | Grain oriented silicon steel plate of low core loss and its manufacture |
| CN1244597A (en) * | 1998-08-07 | 2000-02-16 | 东北大学 | Laser treatment method of orienting the surface of silicon steel |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104217844A (en) * | 2014-09-03 | 2014-12-17 | 南阳市力矩软磁材料科技有限公司 | Silicon steel sheet with low iron loss, low noise, high magnetic flux and high laminating speed and preparation method thereof |
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Address after: 032700 the riverside road north of hhun County, Jinzhong, Shanxi Patentee after: Shanxi silver Saint Technology Co., Ltd. Address before: 032700 the riverside road north of hhun County, Jinzhong, Shanxi Patentee before: Heshun Yinsheng Chemical Co., Ltd. |
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